JP2018519267A - Composite powder obtained by impregnating porous polymer with straw powder particles, cosmetic composition containing the same, and method for producing the same - Google Patents

Composite powder obtained by impregnating porous polymer with straw powder particles, cosmetic composition containing the same, and method for producing the same Download PDF

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JP2018519267A
JP2018519267A JP2017559068A JP2017559068A JP2018519267A JP 2018519267 A JP2018519267 A JP 2018519267A JP 2017559068 A JP2017559068 A JP 2017559068A JP 2017559068 A JP2017559068 A JP 2017559068A JP 2018519267 A JP2018519267 A JP 2018519267A
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powder
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JP2018519267A5 (en
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イ・ヒョンソク
ペク・ドンヒョン
チョ・ガヨン
キム・ヒョンジュン
チョン・ヘジン
チャン・ドンヒョク
キム・ヨンジン
クォン・イギョン
イ・ジョンファン
チェ・ソンウク
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241Containing particulates characterized by their shape and/or structure
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    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
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    • A61K8/0241Containing particulates characterized by their shape and/or structure
    • A61K8/0279Porous; Hollow
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    • A61K8/0283Matrix particles
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8141Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • A61K8/8147Homopolymers or copolymers of acids; Metal or ammonium salts thereof, e.g. crotonic acid, (meth)acrylic acid; Compositions of derivatives of such polymers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8141Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • A61K8/8152Homopolymers or copolymers of esters, e.g. (meth)acrylic acid esters; Compositions of derivatives of such polymers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/817Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Compositions or derivatives of such polymers, e.g. vinylimidazol, vinylcaprolactame, allylamines (Polyquaternium 6)
    • A61K8/8176Homopolymers of N-vinyl-pyrrolidones. Compositions of derivatives of such polymers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/817Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Compositions or derivatives of such polymers, e.g. vinylimidazol, vinylcaprolactame, allylamines (Polyquaternium 6)
    • A61K8/8182Copolymers of vinyl-pyrrolidones. Compositions of derivatives of such polymers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/85Polyesters
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/008Preparations for oily skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/60Particulates further characterized by their structure or composition
    • A61K2800/65Characterized by the composition of the particulate/core
    • A61K2800/654The particulate/core comprising macromolecular material
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/83Electrophoresis; Electrodes; Electrolytic phenomena

Abstract

本発明は、翡翠の粉末と多孔性高分子の複合粉体に係り、より詳しくは、多孔性高分子を溶解させた溶液に翡翠の粉末を分散させた分散液を単一工程(One−step)で噴霧して製造される翡翠の粉末粒子が、多孔性高分子に含浸(Impregnation)された複合粉体(Jade sphere)、これを含む化粧料組成物及びこの製造方法に関するものである。The present invention relates to a composite powder of soot powder and a porous polymer. More specifically, the present invention relates to a single-step (One-step) dispersion of a soot powder in a solution in which a porous polymer is dissolved. The present invention relates to a composite powder impregnated with porous polymer (Jade sphere), a cosmetic composition containing the same, and a method for producing the same.

Description

本出願は、2015年6月30日付け韓国特許出願第10−2015−0092868号と2016年6月27日付け韓国特許出願第10−2016−0080232号に基づいた優先権の利益を主張し、該韓国特許出願の文献に開示された全ての内容は本明細書の一部として含む。   This application claims the benefit of priority based on Korean Patent Application No. 10-2015-0092868 dated June 30, 2015 and Korean Patent Application No. 10-2016-0080232 dated June 27, 2016, All contents disclosed in the document of the Korean patent application are included as part of this specification.

本発明は、翡翠の粉末と多孔性高分子の複合粉体に係り、より詳しくは、多孔性高分子を溶解した溶液に翡翠の粉末を分散させた分散液を単一工程(One−step)で噴霧して製造される翡翠の粉末粒子が多孔性高分子に含浸された複合粉体(Jade sphere)、これを含む化粧料組成物及びこの製造方法に関する。   The present invention relates to a composite powder of soot powder and a porous polymer, and more specifically, a single step (One-step) of a dispersion in which soot powder is dispersed in a solution in which a porous polymer is dissolved. In particular, the present invention relates to a composite powder (Jade sphere) in which a porous polymer is impregnated with powder particles of candy produced by spraying, a cosmetic composition containing the same, and a method for producing the same.

有機粉体と無機粉体の結合体のように、2種以上の粉体が結合された複合粉体を製造する際に、母体となる粉体粒子(A)を製造した後、その表面を別の粉体粒子(B)がコーティングする工程を通じて製造する方法が一般的であるが、このような技術は、2段階の製造工程によって手続きが複雑なだけでなく、2種以上の粉体それぞれの特性がまともに発揮できない問題点があった。一方、粉末化方法の中で噴霧乾燥工程と電気噴霧工程を適用して複合粉体を製造すれば、母体となる粉体粒子(A)内部の間に別の粉体粒子(B)が均一に分散されて浸透しながら単一工程で顆粒粉末を製造できる差がある。   When manufacturing a composite powder in which two or more kinds of powders are combined, such as a combined body of an organic powder and an inorganic powder, after manufacturing the powder particles (A) as a base, A method of manufacturing through a process of coating with another powder particle (B) is generally used, but such a technique is not only complicated by a two-stage manufacturing process but also two or more kinds of powders. There was a problem that the characteristics of this could not be demonstrated properly. On the other hand, if a composite powder is manufactured by applying the spray drying process and the electrospray process in the pulverization method, another powder particle (B) is uniform between the powder particles (A) as a base. There is a difference that a granular powder can be produced in a single step while being dispersed and permeated in a single process.

噴霧乾燥(Spray Drying)技術は、原料粉末、溶媒及びバインダーなどによって構成される溶解状態の物質をノズルや回転ディスクなどの噴霧部で噴霧し、熱風で瞬間的に乾燥する方法である。より具体的に説明すれば、噴霧乾燥は溶液(Solution)、エマルジョン(Emulsion)、分散液(Dispersion)、懸濁液(Suspension)、スラリー(Slurry)などの液状原料を微粒化し、表面積を増加して受熱面積を大きくした後、熱風気流と直接接触することによって、瞬間的に乾燥され液状原料から直ぐ粒状の製品を得る技術であって、乾燥粉末化が単一段階でなされる特徴がある。   The spray drying technique is a method in which a dissolved substance composed of raw material powder, a solvent, a binder, and the like is sprayed by a spraying unit such as a nozzle or a rotating disk, and dried instantaneously with hot air. More specifically, spray drying increases the surface area by atomizing liquid raw materials such as solutions, emulsions, dispersions, suspensions, and slurries. This is a technique for obtaining a granular product immediately dried from a liquid raw material by direct contact with a hot air stream after enlarging the heat receiving area, and is characterized by dry powdering in a single stage.

したがって、製品が熱に接触される時間が数秒内であって製品の物性に比較的に少ない影響を及ぼすという長所と、生産された製品の取り扱いが容易である、などの理由によりファインセラミックス、粉乳、医薬品、食品類、染料及び顔料などを製造する際に、天然抽出物などを乾燥して顆粒を得るために幅広く使われている。   Therefore, fine ceramics and powdered milk have the advantages that the product is in contact with heat within a few seconds and has a relatively small effect on the physical properties of the product, and that the produced product is easy to handle. In manufacturing pharmaceuticals, foods, dyes and pigments, they are widely used to obtain granules by drying natural extracts.

韓国公開特許出願第2002−0091779号には、樹脂に対する分散性、充填性に優れたセラミックス粉末を製造するために、原料粉体を含むスラリーを噴霧して液滴を形成した後、乾燥してセラミックス顆粒粉を得る噴霧乾燥工程について公知されており、韓国公開特許出願第2014−0110439号には、噴霧乾燥工法を利用して一定の粒度を有する球状の窒化ホウ素粉末を製造する方法が公知されている。   In Korean Published Patent Application No. 2002-0091797, in order to produce a ceramic powder with excellent dispersibility and filling properties for resin, a slurry containing raw material powder is sprayed to form droplets and then dried. A spray drying process for obtaining ceramic granule powder is known, and Korean Published Patent Application No. 2014-0110439 discloses a method for producing spherical boron nitride powder having a certain particle size by using a spray drying method. ing.

一方、電気噴霧(Electro−Spraying)技術は、ある程度の電気伝導度と粘度を持つ高分子溶液などを毛細管に注入した後、静電気力を加えて微細粒子を製造する方法である。一般に、垂直に位置したノズルを通じて高分子溶液を噴射させれば、ノズルの先端には重力と高分子溶液の表面張力が均衡を成して半球状の滴を形成して吊られるようになる。このとき、電場が加えられると、この半球状の滴の表面に電荷または双極子配向が空気層と溶液の界面に誘導され、このような電荷や双極子の反発力で表面張力とは反対の力が発生される。したがって、ノズル先端の半球状表面はテイラコーン(Taylor cone)と呼ばれる円錐型表面に増えることになり、電荷や双極子らの反発力が表面張力を克服できるような力以上になれば、荷電された高分子溶液がテイラコーンから放出される。このとき、粘度の低い高分子溶液の場合は、表面張力によって微細な滴として噴射されるようになる。電気噴霧もまた噴霧乾燥と同様に粉末化が単一段階からなる。   On the other hand, the electro-spraying technique is a method for producing fine particles by injecting a polymer solution having a certain degree of electrical conductivity and viscosity into a capillary and then applying electrostatic force. In general, when a polymer solution is ejected through a vertically positioned nozzle, gravity and the surface tension of the polymer solution are balanced to form a hemispherical drop at the tip of the nozzle. At this time, when an electric field is applied, a charge or dipole orientation is induced on the surface of the hemispherical droplet at the interface between the air layer and the solution, and the repulsive force of such charge or dipole is opposite to the surface tension. Force is generated. Therefore, the hemispherical surface at the tip of the nozzle will increase to a conical surface called Taylor cone, and if the charge or the repulsive force of the dipoles exceeds the force that can overcome the surface tension, it will be charged. A polymer solution is released from the Taylor cone. At this time, in the case of a polymer solution having a low viscosity, it is ejected as fine droplets due to surface tension. Electrospraying also consists of a single stage of powdering, similar to spray drying.

電気噴霧は、装置の形態と構造が簡単で、製作が容易であり、発生された粒子が単分散分布を持つだけでなく、数十ナノから数百ミクロまで多様な大きさの粒子を製造するに有用であり、薄膜付着や金属表面へのコーティング、タンパク質と生化学物質などの質量分析や構造解釈などの分野で広く利用されてきた。   Electrospray has a simple device configuration and structure, is easy to manufacture, and the generated particles not only have a monodisperse distribution, but also produce particles of various sizes from tens of nano to hundreds of micro It has been widely used in fields such as thin film deposition, coating on metal surfaces, mass spectrometry of proteins and biochemicals, and structural interpretation.

最近は、薬物伝達分野で薬物を含む粒子生成に適用しようとする研究が進められていて、韓国登録特許第10−1471280号には難溶性薬物の体内吸収率を向上させるために、難溶性物質を有機溶媒に溶解した後、界面活性剤を分散して製造された難溶性物質溶液を電気噴霧して超微粒子難溶性物質のナノ粉体を製造する方法が公知されている。   Recently, research to apply to the production of particles containing drugs in the field of drug delivery has been advanced, and Korean Registered Patent No. 10-1471280 discloses a poorly soluble substance in order to improve the absorption rate of a poorly soluble drug in the body. There is known a method for producing nano-powder of an ultrafine particle poorly soluble substance by electrospraying a hardly soluble substance solution produced by dispersing a surfactant in an organic solvent and then dispersing the surfactant.

本発明者らは、上記噴霧乾燥及び電気噴霧技術が、単一工程で液状原料を顆粒化することができ、顆粒の粒度を調節し易いだけなく、球状の粒子を製造できる点に着目して、噴霧乾燥及び電気噴霧工程を利用して多孔性高分子に無定形の荒い翡翠の粉末粒子を均一に含浸させる技術である本発明に至るようになった。   The inventors pay attention to the fact that the above spray drying and electrospray techniques can granulate a liquid raw material in a single step, not only easily adjust the particle size of the granules, but also produce spherical particles. The present invention has come to the present invention, which is a technique for uniformly impregnating a porous polymer with amorphous rough soot powder particles using spray drying and electrospraying processes.

韓国登録特許第10−1015386号「噴霧乾燥器(Spray Dryer)」Korean Registered Patent No. 10-1015386 “Spray Dryer”

翡翠の粉末粒子は、皮膚保湿や美白効果などを目的として化粧料組成物に含まれる技術が公知されているが、剤形化して皮膚に塗布すると、その表面が荒いから使用感を低下することになる。また、翡翠の粉末粒子が固まることによって白濁現象が発生し、メーキャップ化粧料を含む時、翡翠自体の濁った彩度によって白色度が低下する問題点があった。   The powder particles of candy are known to be contained in cosmetic compositions for the purpose of moisturizing skin and whitening skin. However, when they are formulated and applied to the skin, the surface is rough and the feeling of use is reduced. become. In addition, white turbidity occurs due to the solidification of the powder particles of the cocoon, and when makeup cosmetics are included, there is a problem that the whiteness decreases due to the turbid saturation of the cocoon itself.

このような問題点を解決するために、本発明では多孔性高分子を溶解した溶液に翡翠の粉末を分散した後、噴霧乾燥(Spray Drying)または電気噴霧(Electro−Spraying)の単一工程(One−step)で分散液を噴霧することにより、翡翠の粉末粒子を多孔性高分子に均一に含浸(Impregnation)させた複合粉体(以下、翡翠の含浸粉体、Jade sphere)、これを含む化粧料組成物及びこの製造方法を開示する。   In order to solve such a problem, in the present invention, after the powder of soot is dispersed in a solution in which a porous polymer is dissolved, a single step of spray drying (Electro Spraying) or electro-spraying (Electro-Spraying) A composite powder (hereinafter referred to as Jade sphere), in which the soot powder particles are uniformly impregnated into the porous polymer by spraying the dispersion with One-step), including this A cosmetic composition and a method for producing the same are disclosed.

上記翡翠の粉末の粒子は、10000〜20000meshで、全体複合粉体の重量に対し10〜90重量%、好ましくは50〜90重量%で含浸されてもよい。   The soot powder particles may be impregnated at 10,000 to 20,000 mesh and 10 to 90% by weight, preferably 50 to 90% by weight, based on the weight of the total composite powder.

上記多孔性高分子は、ポリメチルメタクリレート[PMMA:poly−(methyl methacrylate)]、ポリビニルピロリドン[PVP:poly−(vinyl pyrrolidone)]、ポリカプロラクトン[PCL:poly−(caprolactone)] 及びポリ−L−乳酸[PLLA:Poly−(L−Lactic Acid)] 群から選ばれることが望ましい。   The porous polymer includes polymethyl methacrylate [PMMA: poly- (methyl methacrylate)], polyvinylpyrrolidone [PVP: poly- (vinyl pyrrolidone)], polycaprolactone [PCL: poly- (caprolactone)] and poly-L-. The lactic acid is preferably selected from the group [PLLA: Poly- (L-Lactic Acid)].

本発明の翡翠の粉末粒子を多孔性高分子に均一に含浸させた翡翠の含浸粉体(Jade sphere)を化粧料組成物として剤形化すれば、翡翠の粉末が単独で含まれた化粧料より翡翠の粉末のブルーライト遮断効果と、多孔性高分子の皮脂吸着力による化粧持続性が向上する。   Cosmetics containing the cocoon powder alone when the candy impregnated powder (Jade sphere) obtained by uniformly impregnating the porous polymer with the cocoon powder particles of the present invention is formulated as a cosmetic composition The blue light blocking effect of the more candy powder and the makeup sustainability by the sebum adsorption power of the porous polymer are improved.

また、荒い無定形の翡翠の粉末を球状の多孔性高分子の内部に含浸させることにより、塗り性、広がり性及び柔らかさが改善され、固まる現象を解消して白濁現象が防止されるし、白色度が改善される効果がある。   In addition, by impregnating the inside of the spherical porous polymer with rough amorphous cocoon powder, the paintability, spreadability and softness are improved, the phenomenon of solidification is eliminated, and the clouding phenomenon is prevented, There is an effect that the whiteness is improved.

本発明に適用される翡翠の粉末の走査電子顕微鏡(SEM)イメージである。It is a scanning electron microscope (SEM) image of the soot powder applied to this invention. 走査電子顕微鏡(SEM)イメージであって、(a)は本発明の翡翠の含浸粉体表面のイメージで、(b)は切断面のイメージである。It is a scanning electron microscope (SEM) image, (a) is an image of the impregnated powder surface of the soot of the present invention, and (b) is an image of a cut surface. エネルギー分散型X線(EDX:Energy Dispersive X−ray)分析装置であって、定量及び定性分析したイメージであって、(a)は本発明の翡翠の含浸粉体表面のイメージで、(b)は翡翠の含浸粉体に含まれた各元素を可視化したイメージである。An energy dispersive X-ray (EDX) analyzer, which is an image obtained by quantitative and qualitative analysis, wherein (a) is an image of the surface of the impregnated powder of the present invention, (b) Is an image that visualizes each element contained in the impregnated powder of soot. 本発明の翡翠の含浸粉体の可視光線領域帯別反射率(%)テストの結果である。It is the result of the reflectance (%) test according to visible light region band of the impregnated powder of the present invention. 本発明の翡翠の含浸粉体の白色度(whiteness、%R)テストの結果である。It is a result of the whiteness (whiteness,% R) test of the impregnated powder of the present invention. 本発明の翡翠の含浸粉体の吸油量(mL/g)テストの結果である。It is the result of the oil absorption amount (mL / g) test of the impregnated powder of the present invention. 本発明の翡翠の含浸粉体を含む剤形の可視光線領域帯別反射率(%)テストの結果である。It is a result of the reflectance (%) test according to visible light region band of the dosage form containing the soot impregnated powder of the present invention. 本発明の翡翠の含浸粉体を含む剤形の白色度(whiteness、%R)テストの結果である。FIG. 6 is a result of whiteness (% R) test of a dosage form containing the soot impregnated powder of the present invention. FIG.

本発明は、翡翠の粉末と多孔性高分子の複合粉体に係り、より詳しくは、多孔性高分子を溶解した溶液に翡翠の粉末を分散させた後、噴霧乾燥(Spray Drying)または電気噴霧(Electro−Spraying)の単一工程(One−step)で分散液を噴霧することで翡翠の粉末粒子を多孔性高分子に均一に含浸(Impregnation)させた複合粉体(以下、翡翠の含浸粉体、Jade sphere)、これを含む化粧料組成物及びこの製造方法に関する。本発明における「含浸」の意味は、母体となる粉体粒子内部の間に別の粉体粒子が均一に分散して浸透された状態を意味することで、従来の粉体粒子表面を別の粉体粒子がコーティングしたり、粉体表面の気孔の間に担持された形態とは相違する。以下、本発明を詳しく説明する。   The present invention relates to a composite powder of soot powder and a porous polymer, and more specifically, after the soot powder is dispersed in a solution in which the porous polymer is dissolved, spray drying or electrospraying is performed. (Electro-Spraying) A composite powder (hereinafter referred to as soot impregnated powder) in which soot powder particles are uniformly impregnated into a porous polymer by spraying the dispersion in a single step (One-step) Body, Jade sphere), a cosmetic composition containing the same, and a method for producing the same. The meaning of “impregnation” in the present invention means a state in which other powder particles are uniformly dispersed and infiltrated between the inside of the base powder particles, so that the surface of the conventional powder particles is separated from another. It is different from a form in which powder particles are coated or supported between pores on the powder surface. The present invention will be described in detail below.

翡翠(Jade)
一般に、翡翠(Jade)は硬玉(Jadeite jade)と軟玉(Nephrite jade)に分類されるが、軟玉は硬玉におけるナトリウム(Na)とアルミニウム(Al)の組成分とは違い、人体に有益な3つの鉱物、すなわち、カルシウム(Ca)、鉄(Fe)、マグネシウム(Mg)を主成分としている。したがって、本発明に適用できる翡翠の粉末は、その種類に制限されることはないが、より好ましくは軟玉を使用する。
Jade
In general, jade is classified into jadeite jade and nephrite jade, but softball is different from the composition of sodium (Na) and aluminum (Al) in hardball, and is beneficial to the human body. The main component is a mineral, that is, calcium (Ca), iron (Fe), and magnesium (Mg). Therefore, the koji powder that can be applied to the present invention is not limited to the kind thereof, but soft balls are more preferably used.

また、本発明で使われる春川玉は、軟玉の一種として、江原道春川地域で生産される良質の軟玉(Nephrite Jade)で、角閃石(Amphibole)グループの透閃石(Tremolite)と緑閃石(Actinolite)の変種鉱物であるため、その組職が緻密且つ纎細であり、靭性の強い羊毛状組職を持つ鉱物である。   The Chuncheon jade used in the present invention is a high quality Nephrite Jade produced in the Chuncheon area of Gangwon-do as a kind of soft jade. ) Is a mineral that has a fine and fine structure and a strong tough wool structure.

本発明における翡翠は、研磨して粉末に加工されたものを使い、当業者が実施する通常の方法であって軟玉の粉末化方法には制限がない。ただし、本発明において、化粧料組成物として使用できる翡翠の粉末粒子の粒度分布は、10000〜20000meshになるように加工することが望ましい。20000meshを超えると翡翠の粉末効果が微々たるものであり、10000mesh未満であると球状の翡翠の含浸粉体表面が荒くなって、皮膚へ適用する際に使用感が低下するためである。   The wrinkles in the present invention are those that are polished and processed into powder, and are ordinary methods implemented by those skilled in the art, and there is no limitation on the method for pulverizing soft beads. However, in this invention, it is desirable to process so that the particle size distribution of the powder particle | grains of the candy which can be used as a cosmetic composition will be 10000-20000 mesh. If it exceeds 20000 mesh, the powder effect of the wrinkles will be insignificant, and if it is less than 10,000 mesh, the surface of the impregnated powder of spherical wrinkles will become rough, and the feeling of use will be reduced when applied to the skin.

多孔性高分子(Porous Polymer)
本発明において、上記翡翠の粉末粒子が含浸される多孔性高分子は、オイル吸油力と皮脂吸着力を持つ球状(Sphere)粉末状であって、例えば、ポリメチルメタクリレート[PMMA:poly (methyl methacrylate)]を適用したが、この他にもポリビニルピロリドン[PVP:poly (vinyl pyrrolidone)]、ポリカプロラクトン[PCL:poly (caprolactone)] 及びポリ−L−乳酸[PLLA:Poly (L−Lactic Acid)] 群から選ばれることができ、これに制限されないことは勿論である。
Porous polymer
In the present invention, the porous polymer impregnated with the soot powder particles is in the form of a sphere powder having oil absorption and sebum adsorption, such as polymethyl methacrylate [PMMA: poly (methyl methacrylate). In addition, polyvinylpyrrolidone [PVP: poly (vinyl pyrrolidone)], polycaprolactone [PCL: poly (caprolactone)] and poly-L-lactic acid [PLLA: Poly (L-Lactic Acid)] Of course, it can be selected from a group and is not limited thereto.

このような多孔性高分子は粒子の形が球状であるため、様々な化粧料剤形の製造時に配合し易いし、皮膚の上で球状微粒子がローリング(Rolling)されることで皮膚へ塗布する際に塗り性などの使用感が優れており、球状表面の特性である光散乱を利用した皮膚のてかり防止効果と化粧持続性の向上効果によって、通常の皮脂コントロールのための基礎化粧品と皮膚トーンを補正するためのメーキャップ製品に多く使われる。   Since such a porous polymer has a spherical particle shape, it can be easily blended in the production of various cosmetic dosage forms, and is applied to the skin by rolling the spherical fine particles on the skin. Basic cosmetics and skin for regular sebum control due to the excellent anti-painting feeling and the effect of preventing the skin from taking advantage of the light scattering characteristic of the spherical surface and the effect of improving makeup persistence. Often used in makeup products to correct tones.

翡翠の含浸粉体
本発明の翡翠の含浸粉体、すなわち翡翠の粉末粒子が多孔性高分子に均一に含浸された複合粉体において、翡翠の粉末含量は全翡翠の含浸粉体重量に対して10〜90重量%で含浸されてもよく、より好ましくは50〜90重量%で含浸されてもよい。また、翡翠の含浸粉体の平均粒径は5〜20μmであってもよい。このような特徴は、翡翠の粉末による効果と皮膚への適用時の使用感において化粧料として適用することに適切である。
Soot impregnated powder In the soot impregnated powder of the present invention, that is, in the composite powder in which the soot powder particles are uniformly impregnated into the porous polymer, the soot powder content is based on the total weight of the soot impregnated powder. It may be impregnated at 10 to 90% by weight, more preferably 50 to 90% by weight. The average particle size of the soot impregnated powder may be 5 to 20 μm. Such a feature is appropriate for application as a cosmetic in terms of the effect of wrinkle powder and the feeling of use when applied to the skin.

本発明は、翡翠の粉末を多孔性高分子溶液に分散した多孔性高分子分散液を噴霧乾燥(Spray Drying)または電気噴霧(Electro−Spraying)して単一工程(One−step)で翡翠の含浸粉体を製造することであって、翡翠の粉末を多孔性高分子の内部に均一に含浸させることができる。このとき、多孔性高分子の超撥水性を実現するために乳化剤は排除することが望ましい。従来、乳化重合のような方法で生産される多孔性粉体は、乳化剤の使用が不可避であったが、その後の乳化剤の完全除去が不可能であったため皮膚への刺激があり、皮膚の油分だけではなく水分も吸収するので、皮膚が乾燥する問題点があった。しかし、本発明によれば、乳化剤による皮膚刺激がなく、超撥水性を実現して油分のみを選択的に吸収して化粧持続力を高めることができる。   In the present invention, a porous polymer dispersion obtained by dispersing a powder of soot in a porous polymer solution is spray-dried (Spray Drying) or electro-sprayed (Electro-Spraying), and the soot is formed in a single step (One-step). The impregnation powder is produced, and the soot powder can be uniformly impregnated inside the porous polymer. At this time, it is desirable to eliminate the emulsifier in order to achieve super water repellency of the porous polymer. Conventionally, the use of emulsifiers is unavoidable for porous powders produced by methods such as emulsion polymerization, but since the subsequent removal of the emulsifiers is impossible, there is irritation to the skin and the oil content of the skin. Not only does it absorb moisture, it also has the problem of dry skin. However, according to the present invention, there is no skin irritation caused by the emulsifier, and super water repellency can be realized, and only the oil can be selectively absorbed to enhance the makeup sustainability.

また、多孔性高分子溶液は、ポリメチルメタクリレート(PMMA)をジクロロメタン(DCM)とヘキサノール(Hexanol)の混合溶媒に溶解し、ジクロロメタン(DCM)とヘキサノール(Hexanol)の混合比(重量比)は9:1〜7:3の範囲内で選択することができる。ヘキサノールは多孔性高分子のポア(Pore)を形成する役割をするので、ヘキサノールの割合が全溶媒の10重量%未満であれば、ポアのサイズが小さすぎるし、30重量%以上であれば、ポアのサイズが大きすぎて適合しない。   The porous polymer solution is prepared by dissolving polymethyl methacrylate (PMMA) in a mixed solvent of dichloromethane (DCM) and hexanol (Hexanol), and the mixing ratio (weight ratio) of dichloromethane (DCM) and hexanol (Hexanol) is 9 : 1 to 7: 3 can be selected. Since hexanol serves to form a porous polymer pore, if the proportion of hexanol is less than 10% by weight of the total solvent, the pore size is too small, and if it is 30% by weight or more, The pore size is too large to fit.

本発明における翡翠の含浸粉体は、製造工程条件によって気孔特性の制御が可能である。制御できる気孔特性としては、平均気孔サイズ、孔隙率及び全ての気孔の面積などがある。具体的に、平均気孔サイズは15〜800nm、より好ましくは250〜600nmであってもよく、孔隙率は40〜85%、より好ましくは50〜75%であってもよい。また、全ての気孔の面積は1〜100m/g、より好ましくは5〜80m/gである。 The impregnated powder of soot according to the present invention can control the pore characteristics depending on the production process conditions. Pore characteristics that can be controlled include average pore size, porosity, and area of all pores. Specifically, the average pore size may be 15 to 800 nm, more preferably 250 to 600 nm, and the porosity may be 40 to 85%, more preferably 50 to 75%. Moreover, the area of all the pores is 1-100 m < 2 > / g, More preferably, it is 5-80 m < 2 > / g.

このような特徴を持つ翡翠の含浸粉体は、その気孔サイズ及び孔隙率によって吸油量の増大効果を引き起こすことができる。吸油量は後述する水銀の浸透体積(Intrusion Volume)で説明可能である。本発明による翡翠の含浸粉体の水銀浸透体積は0.5〜5cm/gの範囲で測定され、この値は高い信頼水準で吸油量として見做されることがある。 The soot impregnated powder having such characteristics can increase the oil absorption depending on the pore size and porosity. The amount of oil absorption can be explained by the mercury penetration volume (Intrusion Volume) described later. The mercury penetration volume of the soot impregnated powder according to the present invention is measured in the range of 0.5 to 5 cm 3 / g, and this value may be regarded as an oil absorption amount with a high confidence level.

従来の多孔性高分子は、単一大きさのメソポーラス(Meso−Porous)構造によって比表面積が相対的に大きいものの、平均気孔サイズと孔隙率が低いことに対し、本発明の翡翠の含浸粉体の場合は、マルチポーラス(Multi−Porous、Micro+Meso+Macro)構造によってポアチャンネル(Pore Channel)が形成され、毛細管現象によってオイルを吸油することにもっと有利である。   The conventional porous polymer has a relatively large specific surface area due to a single-size meso-porous structure, but has a low average pore size and low porosity. In the case of (1), a pore channel (Pore Channel) is formed by a multi-porous (Multi-Porous, Micro + Meso + Macro) structure, which is more advantageous in absorbing oil by capillary action.

化粧料組成物
上記翡翠の含浸粉体は、化粧料組成物として適用することが可能であり、このとき、上記翡翠の含浸粉体は全化粧料重量に対して0.1〜5.0重量%含むことが望ましい。翡翠の粉末の含量が多すぎると、化粧原料固有の性質や軟性、及び皮膚へ適用する時の使用感が低下するだけでなく、翡翠が高価であるため製品単価が上昇する問題点が発生する。一方、翡翠の粉末の含量が少なければ、翡翠の粉末による効果を期待できないので好ましくない。
Cosmetic composition The above-described soot impregnated powder can be applied as a cosmetic composition. At this time, the above-described soot impregnated powder is 0.1 to 5.0 weight based on the total cosmetic weight. % Is desirable. If the powder content of the cocoon is too high, not only will the properties and softness inherent to cosmetic ingredients and the feeling of use when applied to the skin be reduced, but there will also be a problem that the unit price of the product will increase due to the high price of the cocoon. . On the other hand, if the content of koji powder is small, the effect of koji powder cannot be expected.

また、本発明の化粧料組成物には、翡翠の粉末の他に皮膚しわの改善、皮膚美白改善、皮膚弾力改善、顔面垂れ改善、皮膚保湿改善、皮膚つや改善、皮膚老化防止(例えば、光老化による皮膚しわ形成及び皮膚硬化抑制)、クマ改善及び皮膚角質改善のような皮膚を改善するための機能性添加物や紫外線を遮断するための機能性添加物または一般的な化粧料組成物に含まれる成分がさらに含まれてもよい。   In addition to wrinkle powder, the cosmetic composition of the present invention includes skin wrinkle improvement, skin whitening improvement, skin elasticity improvement, face sagging improvement, skin moisture retention improvement, skin gloss improvement, skin aging prevention (for example, light Skin wrinkle formation and skin hardening suppression due to aging), functional additives for improving skin such as bear improvement and skin keratin improvement, functional additives for blocking ultraviolet rays, or general cosmetic compositions An included component may be further included.

上記皮膚改善のための機能性添加物として、水溶性ビタミン、脂溶性ビタミン、高分子ペプチド、高分子多糖、スフィンゴ脂質、天然抽出物及び醗酵物質からなった群から選ばれた成分を含むことができる。また、紫外線を遮断するための機能性添加物として、二酸化チタン(TiO:Titanium dioxide)、酸化亜鉛(ZnO:Zinc oxide)、酸化セリウム(CeO:Cerium oxide)のような無機粉体をさらに含むことができる。さらに、上記機能性添加物と共に必要に応じて一般的な化粧料組成物に含まれる成分を配合することができる。 The functional additive for improving the skin may contain a component selected from the group consisting of water-soluble vitamins, fat-soluble vitamins, polymer peptides, polymer polysaccharides, sphingolipids, natural extracts, and fermentation substances. it can. In addition, as a functional additive for blocking ultraviolet rays, an inorganic powder such as titanium dioxide (TiO 2 ), zinc oxide (ZnO), cerium oxide (CeO 2 : Cerium oxide) is further added. Can be included. Furthermore, the component contained in a general cosmetic composition can be mix | blended with the said functional additive as needed.

他に含まれる配合成分としては、油脂成分、保湿剤、エモリアント剤、界面活性剤、有機及び無機顔料、有機粉体、紫外線吸収剤、防腐剤、殺菌剤、酸化防止剤、植物抽出物、pH調整剤、アルコール、色素、香料、血行促進剤、冷感剤、制汗剤、精製水などを挙げられるが、これに制限しないことは勿論である。   Other ingredients included are oil and fat ingredients, moisturizers, emollients, surfactants, organic and inorganic pigments, organic powders, UV absorbers, preservatives, bactericides, antioxidants, plant extracts, pH Examples of such agents include, but are not limited to, regulators, alcohols, dyes, fragrances, blood circulation promoters, cooling agents, antiperspirants, and purified water.

上記翡翠の含浸粉体が含まれた化粧料組成物をスキン、スキンローション、クリーム、セラム、エマルジョン、エッセンス、パウダー、ファンデーション、スプレイ、日焼け止め、マスクパック、ジェルのいずれか一つの形態、より好ましくは、マスクパック、シートパック、睡眠パック、ウォッシュオフパック、ピールオフパックなどで剤形化することができるが、剤形において特別に限定されることなく、目的によって適宜選択して変更することができる。   A cosmetic composition containing the above-mentioned impregnated powder of skin is preferably in the form of any one of skin, skin lotion, cream, serum, emulsion, essence, powder, foundation, spray, sunscreen, mask pack and gel. Can be formulated into a mask pack, a seat pack, a sleep pack, a wash-off pack, a peel-off pack, etc., but is not specifically limited in the dosage form and can be appropriately selected and changed depending on the purpose. .

以下、本発明を実施例及び図面によってより詳しく説明する。しかし、本発明は、下記実施例によって限定されることはなく、本発明の技術的思想範囲内で様々な変形または修正することができることは、この分野における通常の知識を有する者には明白である。   Hereinafter, the present invention will be described in more detail with reference to examples and drawings. However, the present invention is not limited by the following examples, and it is obvious to those skilled in the art that various changes or modifications can be made within the scope of the technical idea of the present invention. is there.

下記実施例1及び実施例2を製造するために、次の[表1]を用意した。   In order to produce the following Example 1 and Example 2, the following [Table 1] was prepared.

Figure 2018519267
Figure 2018519267

<実施例1>
上記[表1]を用意し、下記噴霧乾燥の方法によって翡翠の含浸粉体(以下、Jade Sphere)を製造した。
<Example 1>
The above [Table 1] was prepared, and impregnated powder of soot (hereinafter referred to as Jade Sphere) was produced by the following spray drying method.

噴霧乾燥(Spray−Drying)
1)PMMA 40gを溶媒(DCM:Hexanol = 9:1、wt%)1Lに溶解させた。
2)翡翠の粉末40gをPMMA溶液に入れた後、均質器(Homogenizer)を使って分散させた。
3)翡翠の粉末が分散されたPMMA溶液を下記[表2]の条件で噴霧乾燥した。
Spray-drying
1) 40 g of PMMA was dissolved in 1 L of a solvent (DCM: Hexanol = 9: 1, wt%).
2) 40 g of soot powder was put into the PMMA solution and then dispersed using a homogenizer.
3) The PMMA solution in which the soot powder was dispersed was spray-dried under the conditions shown in [Table 2] below.

Figure 2018519267

4)翡翠の粉末が分散されたPMMA溶液は、噴霧乾燥中に持続的に撹拌器で撹拌させた。
5)噴霧乾燥された翡翠の粉末/PMMA複合粉体粒子を十分洗浄した後、凍結乾燥して残存溶媒を完全に取り除いた後得た。
Figure 2018519267

4) The PMMA solution in which the soot powder was dispersed was continuously stirred by a stirrer during spray drying.
5) The spray-dried soot powder / PMMA composite powder particles were sufficiently washed and then freeze-dried to completely remove the residual solvent.

<実施例2>
上記[表1]を用意し、下記電気噴霧方法によって翡翠の含浸粉体(以下、Jade Sphere)を製造した。
<Example 2>
[Table 1] was prepared, and soot impregnated powder (hereinafter referred to as Jade Sphere) was produced by the following electrospraying method.

電気噴霧(Electro Spraying)
1)PMMA0.4gを溶媒(DCM:Hexanol = 9:1、wt%)10mLに溶解させた。
2)翡翠の粉末0.4gをPMMA溶液に入れた後、超音波粉砕機(Sonicator)を使って分散した。
3)翡翠の粉末が分散されたPMMA溶液を下記[表3]の条件で電気噴霧した。
Electro spraying
1) 0.4 g of PMMA was dissolved in 10 mL of a solvent (DCM: Hexanol = 9: 1, wt%).
2) After putting 0.4 g of koji powder into the PMMA solution, it was dispersed using an ultrasonic grinder (Sonicator).
3) The PMMA solution in which the soot powder was dispersed was electrosprayed under the conditions shown in [Table 3] below.

Figure 2018519267

4)電気噴霧された翡翠の粉末/PMMA複合粉体粒子を十分洗浄した後、凍結乾燥して残存溶媒を完全に取り除いた後得た。
Figure 2018519267

4) The electrosprayed soot powder / PMMA composite powder particles were sufficiently washed and then freeze-dried to completely remove the residual solvent.

<比較例1>
上記[表1]の翡翠の粉末を単独で適用した。
<Comparative Example 1>
The soot powder of [Table 1] above was applied alone.

図1は、比較例1の翡翠の粉末の走査電子顕微鏡(SEM)イメージで、図2は、このような翡翠の粉末が多孔性高分子であるポリメチルメタクリレート(PMMA)粒子の内部に均一に含浸された実施例1の翡翠の含浸粉体の表面(a)及び切断面(b)の走査電子顕微鏡(SEM)イメージである。図1に示すように、無定形の荒い構造を持つ粒子である翡翠の粉末を噴霧乾燥及び電気噴霧方式を適用して、図2のようにポリメチルメタクリレート(PMMA)粒子の内部に均一に含浸させることが可能である。   FIG. 1 is a scanning electron microscope (SEM) image of the soot powder of Comparative Example 1, and FIG. 2 is a uniform view of polymethyl methacrylate (PMMA) particles in which the soot powder is a porous polymer. It is a scanning electron microscope (SEM) image of the surface (a) and cut surface (b) of the impregnated powder of the soot of Example 1 impregnated. As shown in FIG. 1, spray powder and electrospraying method are used to uniformly impregnate polymethylmethacrylate (PMMA) particles as shown in FIG. It is possible to make it.

図3は、エネルギー分散型X線(EDX:Energy Dispersive X−ray)分析装置で定量及び定性分析したイメージであって、実施例1の翡翠の含浸粉体(a)と翡翠の含浸粉体に含まれた各元素をポイントで可視化(b)したイメージである。本発明で適用された春川玉の主な成分である、カルシウム(Ca、Red point)、マグネシウム(Mg、Blue point)イオンを確認することができ、これにより翡翠の粉末がポリメチルメタクリレート(PMMA)全体に均一に含浸されて分布されたことを確認することができる。   FIG. 3 is an image obtained by quantitative and qualitative analysis using an energy dispersive X-ray (EDX) analyzer, and the soot impregnated powder (a) and soot impregnated powder of Example 1 It is the image which visualized (b) each contained element by the point. Calcium (Ca, Red point) and magnesium (Mg, Blue point) ions, which are the main components of Chuncheon ball applied in the present invention, can be confirmed, whereby the powder of straw is polymethyl methacrylate (PMMA) It can be confirmed that the entire material is uniformly impregnated and distributed.

項目別テスト
以下では、噴霧乾燥方法で製造された翡翠の含浸粉体の項目別テストを行った。
Another test The following items were itemized tests impregnated powder jade produced by spray-drying method.

<実験例1> 反射率テスト
色差計(ColorMate、Scinco co, ltd.、韓国)を利用して実験対象の360〜740nm反射率スペクトルを測定した。そして、反射率を測定するためにPCソフトウェアであるColorMasterを使用した。反射率を測定して該当領域での遮断率を計算した。
<Experimental Example 1> Reflectance Test A 360-740 nm reflectance spectrum of an experiment object was measured using a color difference meter (ColorMate, Scinco co, Ltd., Korea). Then, ColorMaster, which is PC software, was used to measure the reflectance. The reflectance was measured to calculate the blocking rate in the corresponding area.

図4に示すように、比較例1の翡翠の粉末と、実施例1の翡翠の含浸粉体はいずれも可視光線領域帯(380〜710nm)での反射率が高く表れているが、特に380nmより長波長領域からは実施例1の翡翠の含浸粉体が比較例1の翡翠の粉末より高い反射率を示した。特に、ブルーライト領域である380〜500nmでは、このような反射率の格差が大きいことから、実施例1の翡翠の含浸粉体が比較例1の翡翠の粉末より高いブルーライト遮断率を示すことを分かる。   As shown in FIG. 4, the soot powder of Comparative Example 1 and the soot impregnated powder of Example 1 both show high reflectance in the visible light region band (380 to 710 nm), but in particular, 380 nm. From a longer wavelength region, the soot impregnated powder of Example 1 showed a higher reflectance than the soot powder of Comparative Example 1. In particular, in the blue light region of 380 to 500 nm, since the difference in reflectance is large, the soot impregnated powder of Example 1 shows a higher blue light blocking rate than the soot powder of Comparative Example 1. I understand.

<実験例2> 白色度(Whiteness、%R)テスト
白色度は色の白い度合を1次元的に表した値であって、上記反射率テストで全可視光線領域のXYZ色差値を元に次のような数式を用いて白色度指数を導き出した。
WI=Y+800(xn−x)+1700(yn−y)<CIE Whiteness >
n=0.3101、Yn=0.3162(C/2゜)、Xn=0.3138、Yn=0.3309(C/2゜)
<Experimental example 2> Whiteness (Whiteness,% R) test Whiteness is a value that represents the degree of whiteness of a color in a one-dimensional manner, and is based on XYZ color difference values in the entire visible light region in the reflectance test. The whiteness index was derived using a mathematical formula such as
WI = Y + 800 (x n −x) +1700 (y n −y) <CIE Whiteness>
X n = 0.3101, Y n = 0.3162 (C / 2 °), X n = 0.3138, Y n = 0.3309 (C / 2 °)

図5に示すように、実施例1の翡翠の含浸粉体の白色度が94%で比較例1の翡翠の粉末の白色度84%より白色度が10%改善された結果を表す。   As shown in FIG. 5, the whiteness of the soot impregnated powder of Example 1 is 94%, and the whiteness of the soot powder of Comparative Example 1 is improved by 10% from the whiteness of 84%.

<実験例3> 孔隙率測定テスト
実施例1の翡翠の含浸粉体の気孔特性を分析するために、水銀(Hg)浸透法分析を行った。Porosimeter(Autopore IV 9500、Micrometrics、Londonderry、NH、USA)を利用して水銀の浸透体積(Intrusion Volume)、平均気孔大きさ(4V/A、V:Volume、A:area)及び孔隙率(Porosity)を測定して[表4]に示す。
<Experimental Example 3> Porosity Measurement Test In order to analyze the pore characteristics of the soot impregnated powder of Example 1, mercury (Hg) penetration analysis was performed. Infiltration volume of mercury (Induction Volume), average pore size (4V / A, V: Volume, A: area) and porosity (Porosity) using Porosimeter (Autopore IV 9500, Micrometrics, London, NH, USA) Are measured and shown in [Table 4].

Figure 2018519267

上記「総浸透体積」は、単位グラム当たり浸透される水銀の量、「総孔面積」は円筒状の面積で表した全ての気孔の面積、「平均孔直径」は全ての気孔サイズの平均値、「0.20psiaにおけるバルク密度」は0.20psiaでサンプルの気孔を含んだ実際密度を意味する。
Figure 2018519267

The above "total penetration volume" is the amount of mercury permeated per gram, "total pore area" is the area of all pores expressed as a cylindrical area, and "average pore diameter" is the average value of all pore sizes “Bulk density at 0.20 psia” means the actual density at 0.20 psia including the pores of the sample.

その結果、実施例1の翡翠の含浸粉体の場合、444.2nmの平均気孔大きさと64.37%の高い孔隙率を確認することができた。   As a result, in the soot impregnated powder of Example 1, an average pore size of 444.2 nm and a high porosity of 64.37% could be confirmed.

<実験例4> 吸油量テスト
秤とペトリ皿(Petri dish)を利用して実施例1の翡翠の含浸粉体を1g測量した後、スポイトを利用して人体の皮脂と類似の物性を持つトリグリセリド(Triglyceride)オイルを落とし、実施例1の翡翠の含浸粉体がしっとり濡れるまで要された吸油量を測定した。この時、スパチュラ(Spatular)を利用してオイルがよく濡れるようにミキシングする。
<Experimental Example 4> Oil Absorption Test After measuring 1 g of the impregnated powder of Example 1 using a balance and a Petri dish, a triglyceride having physical properties similar to human sebum using a dropper (Triglyceride) The oil was dropped and the amount of oil required until the impregnated powder of Example 1 was moistened was measured. At this time, mixing is performed using a spatula so that the oil gets wet well.

図6に示すように、実施例1の翡翠の含浸粉体の吸油量は1.7mL/gであって、上記3.孔隙率測定テストで水銀の浸透体積(Total Intrusion Volume)1.6797mL/gととても類似であり、これはすなわち吸油量測定結果の信頼性を立証する結果であって、また翡翠の粉末に比べて最大5倍以上吸油量が増加したことを確認することができる。これは実施例1の翡翠の含浸粉体が翡翠の粉末を50重量%含んでいるにもかかわらず、大きい気孔サイズと高い孔隙率を維持することで発生する効果である。   As shown in FIG. 6, the oil absorption amount of the soot impregnated powder of Example 1 was 1.7 mL / g, and the above 3. It is very similar to the total penetration volume of 1.6797 mL / g in the porosity measurement test, which is the result of demonstrating the reliability of the oil absorption measurement result and also compared to the powder of soot It can be confirmed that the oil absorption increased by a maximum of 5 times or more. This is an effect generated by maintaining a large pore size and high porosity even though the soot impregnated powder of Example 1 contains 50% by weight of soot powder.

以下、上記実施例1で製造された翡翠の含浸粉体を次の[表5]に記載された造成(重量%)によってエマルジョン形態(マスクパック)で剤形化し、項目別テストを行った。   Hereinafter, the soot impregnated powder produced in Example 1 was formulated into an emulsion form (mask pack) according to the composition (% by weight) described in [Table 5] below, and an itemized test was conducted.

Figure 2018519267
Figure 2018519267

<実験例5> 使用性評価テスト
本発明の比較剤形例1、2及び剤形例1につき、25〜35歳の女性30名を対象にして1日2回ずつ1ヶ月間使わせた後、密着性、広がり性、柔らかさ、粒子の固まり、化粧持続性などの項目を比べることにより、化粧料としての使用性を1〜5点まで評価させ、その結果を下記[表6]に示す。
<Experimental Example 5> Usability Evaluation Test After using the comparative dosage form examples 1 and 2 and dosage form example 1 of the present invention for 30 women aged 25 to 35 years twice a day for one month. By comparing items such as adhesion, spreadability, softness, particle agglomeration, makeup sustainability, etc., the usability as a cosmetic was evaluated up to 1 to 5 points, and the results are shown in [Table 6] below. .

Figure 2018519267

上記[表6]を見れば、春川玉粉末を含んだ比較剤形例2の場合は、翡翠の粉末を全然含まない比較剤形例1に比べて粒子が固まる現象が大きく、密着性、広がり性、柔らかさ及び化粧持続性の全項目に対して低い評価値を示す。一方、翡翠の含浸粉体を含んだ剤形例1では、春川玉粉末を含んだ比較剤形例2に比べて粒子の固まりが大きく減り、密着性、広がり性が改善され、柔らかさと化粧持続性が比較剤形例1と類似したり向上した水準と示された。
したがって、本発明の翡翠の含浸粉体は、球状で起因する柔らかさと、高い孔隙率による皮脂吸油で起因する化粧持続性でも優秀な結果を示す。また、翡翠の粉末を含む比較剤形例2の最大の問題点であった粒子の固まりを大きく改善して白濁現象を防止できることを確認した。
Figure 2018519267

According to the above [Table 6], in the case of the comparative dosage form example 2 containing the Chuncheon ball powder, the phenomenon that the particles are solidified is larger than that of the comparative dosage form example 1 which does not contain any strawberry powder, and the adhesion and spread are large. A low evaluation value is shown for all items of sex, softness and makeup sustainability. On the other hand, in Dosage Form Example 1 containing koji impregnated powder, particle mass is greatly reduced compared to Comparative Dosage Form Example 2 containing Chuncheon Tama powder, adhesion and spreadability are improved, and softness and makeup persistence. The properties were shown to be similar or improved to those of Comparative Dosage Form Example 1.
Accordingly, the impregnated powder of the present invention shows excellent results in the softness caused by the spherical shape and the makeup sustainability caused by the sebum oil absorption due to the high porosity. In addition, it was confirmed that the cloudiness phenomenon can be prevented by greatly improving the particle mass, which was the biggest problem of Comparative Formulation Example 2 containing soot powder.

<実験例6> 剤形の反射率テスト
上記比較剤形例1、2及び剤形例1の剤形の可視光線領域内の遮断率を測定するために、色差計(ColorMate、Scinco co, ltd.、韓国)を利用して実験対象の360〜740nm反射率スペクトルを測定した。そして、反射率を測定するためにPCソフトウェアであるColorMasterを使用した。
<Experimental Example 6> Reflectance Test of Dosage Form In order to measure the blocking rate in the visible light region of the dosage forms of Comparative Dosage Form Examples 1 and 2 and Dosing Form Example 1, a color difference meter (ColorMate, Scinco co, ltd , Korea), the 360-740 nm reflectance spectrum of the test object was measured. Then, ColorMaster, which is PC software, was used to measure the reflectance.

図7に示すように、剤形化された比較剤形例1、2及び剤形例1はいずれも粉末状態の反射率テスト結果と類似に表れたが、特にブルーライト領域の短波長の光であるほど翡翠の含浸粉体を含んだ製造例1の反射率の格差が大きいことから、翡翠の含浸粉体を剤形化しても高いブルーライト遮断率を示すことが分かる。   As shown in FIG. 7, the dosage forms of Comparative Dosage Form Examples 1 and 2 and Dosage Form Example 1 all appear similar to the reflectance test results in the powder state. The larger the difference in the reflectance of Production Example 1 containing soot impregnated powder, the higher the blue light blocking rate even if the soot impregnated powder is formulated.

<実験例7> 剤形の白色度(Whiteness、%R)テスト
剤形の白色度は、色の白い度合を1次元的に表した値であって、上記剤形の反射率テストで全可視光線領域のXYZ色差値を元に次のような数式を用いて白色度指数を導き出した。
<Experimental Example 7> Whiteness (Whiteness,% R) Test of Dosage Form The whiteness of the dosage form is a one-dimensional value representing the degree of whiteness of the color, and is completely visible in the reflectance test of the dosage form. Based on the XYZ color difference values in the light ray region, the whiteness index was derived using the following mathematical formula.

WI=Y+800(xn−x)+1700(yn−y)<CIE Whiteness >
n=0.3101、Yn=0.3162(C/2゜)、Xn=0.3138、Yn=0.3309(C/2゜)
WI = Y + 800 (x n −x) +1700 (y n −y) <CIE Whiteness>
X n = 0.3101, Y n = 0.3162 (C / 2 °), X n = 0.3138, Y n = 0.3309 (C / 2 °)

図8に示すように、翡翠の粉末を含まない比較剤形例1に比べて翡翠の粉末または翡翠の含浸粉体を含んだ比較剤形例2及び剤形例1の白色度が有意的に向上したことが分かるし、微細ではあるが剤形例1の翡翠の含浸粉体の白色度が最も高い水準であることを確認した。   As shown in FIG. 8, the whiteness of Comparative Dosage Form Example 2 and Dosage Form Example 1 containing soot powder or soot impregnated powder is significantly higher than that of Comparative Dosage Form Example 1 containing no soot powder. It was confirmed that the whiteness of the impregnated powder of the dosage form example 1 was the highest, although it was fine.

<剤形例2>
以下、上記実施例1で製造された翡翠の含浸粉体を0.1重量%含み、次の[表7]に記載された造成(重量%)によって通常的な方法で栄養化粧水を製造した。
<Form example 2>
Hereinafter, a nutritional lotion was prepared by a conventional method including 0.1% by weight of the impregnated powder of the candy manufactured in Example 1 and the composition (% by weight) described in [Table 7] below. .

Figure 2018519267
Figure 2018519267

<剤形例3>
以下、上記実施例1で製造された翡翠の含浸粉体を3.0重量%含み、次の[表8]に記載された造成(重量%)によって通常的な方法で栄養クリームを製造した。
<Form example 3>
Hereinafter, a nutritional cream was prepared by a conventional method by 3.0% by weight of the soot impregnated powder produced in Example 1 and by the preparation (% by weight) described in the following [Table 8].

Figure 2018519267
Figure 2018519267

<剤形例4>
以下、上記実施例1で製造された翡翠の含浸粉体を5.0重量%含み、次の[表9]に記載された造成(重量%)によって通常的な方法でマッサージクリームを製造した。
<Form example 4>
Hereinafter, massage cream was produced in a conventional manner by 5.0% by weight of the candy impregnated powder produced in Example 1 above, and by the preparation (% by weight) described in the following [Table 9].

Figure 2018519267
Figure 2018519267

Claims (13)

翡翠(Jade)の粉末粒子が多孔性高分子に含浸(Impregnation)された複合粉体。   A composite powder obtained by impregnating a porous polymer with powder particles of Jade. 上記翡翠の粉末は、全複合粉体重量に対して50〜90重量%で含浸されることを特徴とする請求項1に記載の複合粉体。   2. The composite powder according to claim 1, wherein the soot powder is impregnated at 50 to 90 wt% with respect to the total weight of the composite powder. 上記多孔性高分子は、ポリメチルメタクリレート[PMMA:poly−(methyl methacrylate)]、ポリビニルピロリドン[PVP:poly−(vinyl pyrrolidone)]、ポリカプロラクトン[PCL:poly−(caprolactone)] 及びポリ−L−乳酸[PLLA:Poly−(L−Lactic Acid)] 群から選ばれる1種以上であることを特徴とする請求項1に記載の複合粉体。 The porous polymer includes polymethyl methacrylate [PMMA: poly- (methyl methacrylate)], polyvinyl pyrrolidone [PVP: poly- (vinyl pyrrolidone)], polycaprolactone [PCL: poly- (caprolactone)] and poly-L-. The composite powder according to claim 1, wherein the composite powder is at least one selected from the group consisting of lactic acid [PLLA: Poly- (L-Lactic Acid)]. 上記複合粉体の平均粒径は5〜20μmであることを特徴とする請求項1に記載の複合粉体。   The composite powder according to claim 1, wherein the composite powder has an average particle size of 5 to 20 μm. 上記複合粉体の平均気孔サイズは15〜800nmであることを特徴とする請求項1に記載の複合粉体。   The composite powder according to claim 1, wherein the composite powder has an average pore size of 15 to 800 nm. 上記複合粉体の孔隙率は40〜85%であることを特徴とする請求項1に記載の複合粉体。   The composite powder according to claim 1, wherein the composite powder has a porosity of 40 to 85%. 請求項1ないし請求項6のいずれか一項の複合粉体を含む化粧料組成物。 A cosmetic composition comprising the composite powder according to any one of claims 1 to 6. 上記複合粉体は、全化粧料重量に対して0.1〜5.0重量%含まれることを特徴とする請求項7に記載の化粧料組成物。   The cosmetic composition according to claim 7, wherein the composite powder is contained in an amount of 0.1 to 5.0% by weight based on the total cosmetic weight. 上記化粧料組成物は、スキン、スキンローション、クリーム、セラム、エマルジョン、エッセンス、パウダー、ファンデーション、スプレイ、日焼け止め、マスクパック、ジェルのいずれか一つの形態で剤形化されることを特徴とする請求項7に記載の化粧料組成物。   The cosmetic composition is formulated in any one form of skin, skin lotion, cream, serum, emulsion, essence, powder, foundation, spray, sunscreen, mask pack, and gel. The cosmetic composition according to claim 7. 多孔性高分子溶液に翡翠の粉末を分散させた分散液を噴霧乾燥(Spray Drying)して製造することを特徴とする、翡翠の粉末粒子が多孔性高分子に含浸された複合粉体の製造方法。   Manufacture of a composite powder obtained by impregnating a porous polymer with a powder of cocoon powder, which is produced by spray-drying a dispersion in which the powder of cocoon is dispersed in a porous polymer solution Method. 多孔性高分子溶液に翡翠の粉末を分散させた分散液を電気噴霧(Electro−Spraying)して製造することを特徴とする、翡翠の粉末粒子が多孔性高分子に含浸された複合粉体の製造方法。   A composite powder obtained by impregnating a porous polymer with soot powder particles, which is produced by electro-spraying a dispersion in which soot powder is dispersed in a porous polymer solution. Production method. 上記多孔性高分子溶液は、ポリメチルメタクリレート[PMMA:poly−(methyl methacrylate)]、ポリビニルピロリドン[PVP:poly−(vinyl pyrrolidone)]、ポリカプロラクトン[PCL:poly−(caprolactone)] 及びポリ−L−乳酸[PLLA:Poly−(L−Lactic Acid)] 群から選ばれる1種以上の高分子を溶媒に溶解させたもので、
上記溶媒は、ジクロロメタンとヘキサノールの混合溶媒であることを特徴とする、請求項10または請求項11に記載の複合粉体の製造方法。
The porous polymer solution includes polymethyl methacrylate [PMMA: poly- (methyl methacrylate)], polyvinylpyrrolidone [PVP: poly- (vinyl pyrrolidone)], polycaprolactone [PCL: poly- (caprolactone)] and poly-L. -Lactic acid [PLLA: Poly- (L-Lactic Acid)] One or more polymers selected from the group are dissolved in a solvent,
The method for producing a composite powder according to claim 10 or 11, wherein the solvent is a mixed solvent of dichloromethane and hexanol.
上記ジクロロメタンとヘキサノールの重量比は9:1〜7:3であることを特徴とする請求項12に記載の複合粉体の製造方法。   The method for producing a composite powder according to claim 12, wherein the weight ratio of dichloromethane to hexanol is 9: 1 to 7: 3.
JP2017559068A 2015-06-30 2016-06-28 A composite powder in which jade powder particles are impregnated in a porous polymer, a cosmetic composition containing the composite powder, and a method for producing the same. Active JP6796082B2 (en)

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